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Designation: D 5463 03
1. Scope*
1.1 This guide covers general considerations for the use of
test kits for quantitative determination of analytes in water and
wastewater. Test kits are available from various manufacturers
for the determination of a wide variety of analytes in drinking
water, surface or ground waters, domestic and industrial
feedwaters and wastes, and water used in power generation and
steam raising. See Table 1 for a listing of some of the types of
kits that are available for various inorganic analytes in water.2
1.2 Ranges, detection limits, sensitivity, accuracy, and susceptibility to interferences vary from kit to kit, depending on
the methodology selected by the manufacturer. In some cases,
kits are designed to replicate exactly an official test method of
a standard-setting organization such as the Association of
Official Analytical Chemists (AOAC), American Public Health
Association (APHA), ASTM, or the U.S. Environmental Protection Agency (USEPA). In other cases, minor modifications
of official test methods are made for various reasons, such as to
improve performance, operator convenience, or ease of use.
Adjustments may be made to sample size, reagent volumes and
concentrations, timing, and details of the analytical finish. In
yet other cases, major changes may be made to the official test
method, such as the omission of analytical steps, change of the
analytical finish, omission of reagents, or substitution of one
reagent for another. Reagents in test kits are often combined to
obtain a fewer number and make the test easier to use.
Additives may also be used to minimize interferences and to
make the reagent more stable with time. A kit test method may
be based on a completely different technology, not approved by
any official or standard-setting organization. Combinations of
test kitsmulti-parameter test kitsmay be packaged to
satisfy the requirements of a particular application conveniently. The test kits in such combination products may be used
to make dozens of determinations of several parameters.
1
This guide is under the jurisdiction of ASTM Committee D19 on Water and is
the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in
Water.
Current edition approved June 10, 2003. Published July 2003. Originally
approved in 1993. Last previous edition approved in 1998 as D 546398.
2
Test kits for determining inorganic analytes in water are available from various
United States and foreign manufacturers, as well as from laboratory supply
companies.
Annual
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11.01.
11.02.
14.02.
03.06.
D 5463 03
TABLE 1 Availability and Types of Test Kits
Analyte
Kit Methodology A
Acidity
Alkalinity
Aluminum
Ammonia
Boron
Bromine
Cadmium
Calcium
Carbon dioxide
Chloride
Chlorine
Chlorine dioxide
Chromium (III)
Chromium (VI)
Cobalt
Copper
Cyanide
Fluoride
Hardness
Hydrazine
Hydrogen peroxide
Iodine
Iron
Lead
Manganese
Magnesium
Molybdate
Nickel
Nitrate
Nitrite
Oxygen (dissolved)
Ozone
Permanganate
pH
Phosphate
Silica
Silver
Sulfate
Sulfide
Sulfite
Thiocyanate
Tin
Vanadium
Zinc
T
C, P, T
C, P
C, P
C, P
C, P, T
C
P, T
T
A, C, P, T
C, P, T
C, P, T
C
C, P, T
C
C, P, T
C, P, T
P
C, GNG, P, T
C, P
C, P, T
C, P, T
C, P
C, P
C, P
C, T
C, P, T
C, P
C, P
C, P, T
C, P, T
C, P
C, T
C, P
C, P
C, P
P
A, C, P, T
C, P, T
C, P, T
C
C
C
C, P, T
A
Kit Methodology: A = appearance/turbidity, C = visual colorimetric, GNG = go
no go, P = photometric, and T = titrimetric.
3. Terminology
3.1 DefinitionsFor definitions of terms used in this guide,
refer to Terminology D 1129 and Practice D 4691.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 analytethe chemical or constituent being determined.
3.2.2 carryoverthe contamination of a subsequent sample
by a previous sample, typically due to incomplete cleaning of
a reused test kit component.
3.2.3 expiration datea date applied by the manufacturer
after which an accurate result is not ensured by the manufacturer.
3.2.4 finish (usually analytical finish)the analytical methodology used for the measuring step of the analysis.
3.2.5 kit (or test kit)a commercially packaged collection
of components that is intended to simplify the analytical testing
function.
3.2.6 interferencean effect of a matrix component that
might cause an analytical bias or that might prevent a successful analysis.
6. General Considerations
6.1 PersonnelThe selection of a test kit and determination
that the test kit analysis is appropriate should be conducted by
a responsible chemist. The development of suitable protocols
7
Other documents: Offcial Methods of Analysis of the Association of Offcial
Analytical Chemists, 15th Ed., AOAC, Arlington, VA, 1990. Changes are published in annual supplements. Standard Methods for the Examination of Water and
Wastewater, 17th Ed., APHA, AWWA, and WPCF. Washington, DC, 1989. Methods
for the Chemical Analysis of Water and Wastes, USEPA, Cincinnati, OH, March
1983.
8
Spokes, G. Neil, and Bradley, Julie A., Performance Testing of Selected Test
Kits for Analysis of Water Samples, ASTM STP 1102, ASTM, Philadelphia, PA,
1991.
D 5463 03
eter for photo-electric color determinations. The manufacturers photometer may be based on optical filters using either
colored glass or plastic, or on interference filters or LEDs. The
filter bandwidth may be wide (up to 100-nm full width half
maximum height) for colored glass or plastic filters and LEDs
or quite narrow (10 nm) with interference filters. The laboratory spectrophotometer may have a 1- to 20-nm bandwidth and
is typically more accurate than a kit photometer or colorimeter.
Refer to Practices E 275 and E 958 for additional discussion of
colorimetry.
7. Interferences
7.1 Kit chemistries that are based on an official test method
are subject to the same interferences as that test method. If the
kit manufacturer uses a revised version of the official test
method, the revision may increase or decrease interference
effects.
7.2 Sample carryover effects may occur if a common
sampling cup or tube is used. Appropriate care is necessary
under such conditions in order to prevent sample carryover.
The carryover may be prevented or reduced by either cleaning
the reused item or rinsing with fresh sample several times.
Aggressive cleaning action may be necessary after a sample
containing a high concentration is tested.
7.3 Careful note should be made of the manufacturers
comments concerning interferences, and appropriate action
should be taken.
7.4 Temperature may affect kit performance.
8. Apparatus
8.1 Colorimetric DeterminationsMany procedures depend on color determination with a color comparator, photometer, or spectrophotometer. The manufacturer may offer a color
comparator for visual comparisons based on liquid, glass,
plastic, or printed color standards. The manufacturer may offer
a photometer or may recommend the use of a spectrophotom-
9
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD.
D 5463 03
11. Samples and Sampling Procedures
11.1 Sample CollectionUnless otherwise specified, collect all samples in accordance with Specification D 1192 and
Practices D 3370.
11.2 Sample HandlingFollow the kit manufacturers recommended sample handling procedures, when available. Contamination and loss are of prime concern for the determination
of trace metals. Environmental dust and impurities in apparatus
components that contact the sample are potential sources of
contamination. Containers can introduce errors in the measurement of trace metals by contributing contaminants through
leaching or surface desorption or by depleting the concentration of the analyte through adsorption. Refer to Practice
D 4453 for the handling of ultra-pure water samples.
11.3 On-Site SamplingTest kits that permit on-site analysis offer great advantages to their users, inasmuch as errorprone sample preservation techniques are often unnecessary.
However, the value of an analytical result is only as good as the
sample that is obtained, and the usual care is required to ensure
the representativeness of the sample.
11.4 Sample ContainersTake care to collect a representative sample in clean containers that will not cause contamination in any significant way.
11.5 Sample SizeThe sample size shall be sufficient to
complete the determinations. A larger sample may be necessary
when sample processing or multiple determinations, or both,
are required.
11.6 Sample Preservation and StorageThe kit method
ordinarily permits an immediate measurement. If the test result
is equivocal or the responsible chemist directs that a preserved
sample be obtained, preserve a sample in accord with the
applicable approved procedure.
D 5463 03
14.3 Perform sample analysis procedures in accord with the
kit manufacturers instructions.
14.4 The frequency of quality control check samples should
be based on a statistical plan established to achieve a desired
level of confidence. An alternative plan is to check at least one
calibration standard after every 10 samples and at the end of
the analyses. Analyze the quality control check samples, split
samples, and spiked samples as directed by quality control
procedures.
15. Calculation
15.1 In most cases, kit test methods provide instructions that
lead to direct numeric results. The user should follow the
manufacturers instructions.
15.2 UnitsThe numeric results obtained from the test kit
should be stated clearly in commonly used units, for example,
mg/L, g/L, ppm (parts per million), or ppb (parts per billion).
If a result is presented as ppm or ppb, it should specify whether
this is a weight or volume specification. Note that ppm in gas
analyses is almost always volume per volume, whereas ppm in
dissolved gas results usually means mg/L, for example, dissolved oxygen in water. The numeric results should specify the
measurement units where chemical species may vary, for
example, nitrate as nitrogen versus nitrate as nitrate. In the use
of test kits for process control, the analyte may be measured in
terms of a treating chemical, not in mg/L of a particular ion.
15.3 The user should refer to Practice E 178 to deal with
outlying observations.
SUMMARY OF CHANGES
Committee D19 has identified the location of selected changes to this standard since the last issue (D 546398)
that may impact the use of this standard.
(1) The QC Section 13 was modified.
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